CN116854480A - Method for preparing aluminum nitride powder by carbothermic process - Google Patents
Method for preparing aluminum nitride powder by carbothermic process Download PDFInfo
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- CN116854480A CN116854480A CN202310758799.XA CN202310758799A CN116854480A CN 116854480 A CN116854480 A CN 116854480A CN 202310758799 A CN202310758799 A CN 202310758799A CN 116854480 A CN116854480 A CN 116854480A
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- 239000000843 powder Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 31
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 30
- 230000008569 process Effects 0.000 title claims description 11
- 239000000463 material Substances 0.000 claims abstract description 73
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000002994 raw material Substances 0.000 claims abstract description 51
- 238000010438 heat treatment Methods 0.000 claims abstract description 37
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000006229 carbon black Substances 0.000 claims abstract description 10
- 238000011068 loading method Methods 0.000 claims abstract description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 238000007873 sieving Methods 0.000 claims abstract description 4
- 238000009826 distribution Methods 0.000 claims description 32
- 239000007789 gas Substances 0.000 claims description 25
- 238000007790 scraping Methods 0.000 claims description 12
- 230000007246 mechanism Effects 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 7
- 230000009467 reduction Effects 0.000 abstract description 6
- 239000000047 product Substances 0.000 description 8
- 239000000919 ceramic Substances 0.000 description 5
- 238000000498 ball milling Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 3
- 239000008188 pellet Substances 0.000 description 3
- 230000000149 penetrating effect Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000009690 centrifugal atomisation Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B17/00—Furnaces of a kind not covered by any preceding group
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/6265—Thermal treatment of powders or mixtures thereof other than sintering involving reduction or oxidation
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/6268—Thermal treatment of powders or mixtures thereof other than sintering characterised by the applied pressure or type of atmosphere, e.g. in vacuum, hydrogen or a specific oxygen pressure
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D3/00—Charging; Discharging; Manipulation of charge
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
- F27D7/02—Supplying steam, vapour, gases, or liquids
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/46—Gases other than oxygen used as reactant, e.g. nitrogen used to make a nitride phase
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D3/00—Charging; Discharging; Manipulation of charge
- F27D2003/0085—Movement of the container or support of the charge in the furnace or in the charging facilities
- F27D2003/0087—Rotation about a vertical axis
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
- F27D7/02—Supplying steam, vapour, gases, or liquids
- F27D2007/023—Conduits
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27M—INDEXING SCHEME RELATING TO ASPECTS OF THE CHARGES OR FURNACES, KILNS, OVENS OR RETORTS
- F27M2003/00—Type of treatment of the charge
- F27M2003/16—Treatment involving a chemical reaction
- F27M2003/165—Reduction
Abstract
The invention relates to a method for preparing aluminum nitride powder by carbothermic reduction, which comprises the following steps: preparing raw material balls, mixing alumina and carbon black in proportion, loading the mixture into a ball mill for mixing with grinding materials, sieving, and granulating to obtain raw material balls for later use; the prepared raw material balls are put into a heating furnace, a material carrying container is rotatably arranged in the heating furnace, a nitrogen pipeline is communicated with the heating furnace, and the raw material balls are put into the material carrying container; introducing nitrogen into a heating furnace through a nitrogen pipeline, starting the heating furnace to heat objects in the furnace, wherein the heating temperature is 1600-1800 ℃ and the heating time is 3h; collecting the reacted product to a carbon removing device, and introducing air into the carbon removing device, wherein the temperature in the carbon removing device is 600-650 ℃; and collecting the product after the reaction in the carbon removal device to obtain the finished aluminum nitride powder. The method for preparing the aluminum nitride powder by the carbothermic method can promote the raw materials to fully react, and the prepared finished product has high purity.
Description
Technical Field
The invention relates to the technical field of aluminum nitride powder preparation, in particular to a method for preparing aluminum nitride powder by a carbothermic reduction method.
Background
Aluminum nitride ceramics (AIN ceramics) have become ideal packaging and substrate materials for electronic components due to high thermal conductivity, low thermal expansion coefficient, high strength, high corrosion resistance, insulation, low permittivity and other excellent comprehensive properties, and the preparation of aluminum nitride powder has important effects on the sintering, molding, heat conduction efficiency and other properties of the final aluminum nitride ceramics. The method for synthesizing aluminum nitride ceramic powder is many, there are many methods such as aluminum powder direct nitriding method, carbothermic reduction method, chemical vapor deposition method, sol-gel method, self-propagating high-temperature synthesis method and plasma chemical synthesis method at present, wherein the product purity that carbothermic reduction method produced is high, shaping and sintering performance are good, when adopting carbothermic reduction method to prepare aluminum nitride powder, because the raw material ball can not be stirred when being heated in the heating furnace, and the raw material has certain thickness, the raw material ball has the condition of uneven abundant reaction when reacting with nitrogen, and after the thickness that the raw material piles up increases, the reaction degree of raw material and inside raw material on the top layer can produce great difference, lead to the final aluminum nitride powder composition to produce the deviation.
Disclosure of Invention
In order to overcome the technical defects in the prior art, the invention provides a method for preparing powder by a carbothermal reduction method, which can promote the raw materials to fully react and has high purity of the prepared finished product.
The technical scheme adopted by the invention is as follows: the carbothermic process of preparing aluminum nitride powder includes the following steps
S1, preparing raw material balls, mixing alumina and carbon black in proportion, loading the mixture into a ball mill for mixing with grinding materials, sieving, and granulating to obtain the raw material balls for later use;
s2, putting the prepared raw material balls into a heating furnace, wherein a material carrying container is rotatably arranged in the heating furnace, a nitrogen pipeline is communicated with the heating furnace, and the raw material balls are put into the material carrying container;
s3, introducing nitrogen into the heating furnace through a nitrogen pipeline, and starting the heating furnace to heat objects in the furnace, wherein the heating temperature is 1600-1800 ℃ and the heating time is 3 hours;
s4, collecting the reacted product to a carbon removing device, and introducing air into the carbon removing device, wherein the temperature in the carbon removing device is 600-650 ℃;
s5, collecting the product after the reaction in the carbon removal device to obtain the finished aluminum nitride powder.
Preferably, the mass ratio of the alumina to the carbon black is 2:0.6-1.2.
Preferably, 11% by weight of aluminum nitride seed crystal and 5% by weight of sintering aid by weight are added to the raw material pellet composed of aluminum oxide and carbon black.
Preferably, the heating furnace comprises a furnace body, the material carrying container is rotatably arranged at the bottom of the furnace body, a driving mechanism for driving the material carrying container to rotate is arranged outside the furnace body, the inner wall of the material carrying container is connected with a material carrying plate, the upper end of the furnace body is connected with a nitrogen channel communicated with the material carrying container, the inner wall of the material carrying container is connected with a material carrying plate, and the air outlet end of the nitrogen channel is aligned with the material carrying plate.
Preferably, the nitrogen channel comprises an air inlet pipeline penetrating through the top of the furnace body and a porous air distribution plate connected to the lower end of the air inlet pipeline, an air inlet hole communicated with the air inlet pipeline is formed in the upper end of the porous air distribution plate, a plurality of air outlet holes are formed in the lower end of the porous air distribution plate, each air outlet hole is provided with a pyramid, a channel is formed in the pyramid, and the channel is provided with an air inlet end communicated with the air outlet holes and a plurality of air outlet ends distributed on the surface of the pyramid.
Preferably, the material carrying plate is an annular plate, the porous gas distribution plate is a sector plate, the gas inlet holes of the porous gas distribution plate are arranged at the circle center of the sector plate, the material scraping plate is arranged at the bottom end of the porous gas distribution plate and is arranged on one straight edge of the porous gas distribution plate, the bottom end height of the material scraping plate is higher than that of the pyramid, and a plurality of gas outlet holes are distributed along a plurality of arc paths around the circle center of the gas distribution plate.
Preferably, a powder pipeline is arranged on the top of the furnace body in a penetrating way, and the lower end of the powder pipeline is aligned to the top surface of the material carrying plate.
Preferably, the rotating speed of the material carrying container is 0.05r/min-0.1r/min.
The invention has the beneficial effects that: according to the heating furnace, the material carrying container is rotatably arranged in the furnace body of the heating furnace, the inner wall of the material carrying container is connected with the material carrying plate, the upper end of the furnace body is connected with the air inlet pipeline communicated with the material carrying container, the lower end of the air inlet pipeline is connected with the porous gas distribution plate, raw materials are put on the material carrying plate during operation, the driving mechanism drives the material carrying container to rotate, the scraping plate on the porous gas distribution plate pushes the raw materials to form a raw material layer with uniform thickness, meanwhile, the pyramid at the lower end of the porous gas distribution plate enters the raw material layer and injects nitrogen into the raw material layer, the nitrogen can push the raw materials to roll when reacting with the raw materials, so that the nitrogen and various raw materials are in a flowing and mixing state, each reaction component can fully react, and the purity of the product is improved.
Drawings
Fig. 1 is a schematic view of the structure of the heating furnace of the present invention.
Fig. 2 is a partial enlarged view at a in fig. 1.
Fig. 3 is a bottom view of the porous gas distribution plate of the present invention.
FIG. 4 is a top view of the porous gas distribution plate of the present invention.
Fig. 5 is a schematic view of the structure of the pyramid of the present invention.
Reference numerals illustrate: 1. a furnace body; 101. an air intake duct; 1011. a porous gas distribution plate; 10111. an air inlet hole; 10112. an air outlet hole; 1012. a scraping plate; 1013. a pyramid; 10131. an air inlet end; 10132. an air outlet end; 102. a powder conduit; 2. a loading container; 201. a material carrying plate; 202. a driving mechanism.
Detailed Description
The invention is further described below with reference to the accompanying drawings:
as shown in fig. 1 to 5, the present embodiment provides a method for preparing aluminum nitride powder by carbothermic process, comprising the steps of
S1, preparing raw material balls, mixing alumina and carbon black in proportion, loading the mixture into a ball mill for mixing with grinding materials, sieving, and granulating to obtain the raw material balls for later use;
s2, putting the prepared raw material balls into a heating furnace, wherein a material carrying container 2 is rotatably arranged in the heating furnace, a nitrogen pipeline is communicated with the heating furnace, and the raw material balls are put into the material carrying container 2;
s3, introducing nitrogen into the heating furnace through a nitrogen pipeline, and starting the heating furnace to heat objects in the furnace, wherein the heating temperature is 1600-1800 ℃ and the heating time is 3 hours;
s4, collecting the reacted product to a carbon removing device, and introducing air into the carbon removing device, wherein the temperature in the carbon removing device is 600-650 ℃;
s5, collecting the product after the reaction in the carbon removal device to obtain the finished aluminum nitride powder.
In this embodiment, the mass ratio of alumina to carbon black is 2:0.6-1.2, preferably, 11% by weight of aluminum nitride seed crystal and 5% by weight of sintering aid are added to the raw material pellets composed of aluminum oxide and carbon black in the preparation of raw material pellets.
In this embodiment, during granulation, a slurry is obtained after wet ball milling of the powder after ball milling, during wet ball milling, a binder and a dispersing agent are added into the mixture, the mass ratio of the binder to the mixture is 1-5:100, the mass ratio of the dispersing agent to the mixture is 0.1-1:100, a solvent is added during the wet ball milling, the solid content of the obtained slurry is 45% -65%, and centrifugal atomization is performed on the obtained slurry in a stirring state, so that a raw material ball is obtained.
When the average particle size of the alumina powder is too small during sintering, the powder is easy to agglomerate, which is not beneficial to the reaction, and when the average particle size is too large, the porosity of the finally formed aluminum nitride ceramic is too high, so in this embodiment, the average particle size of the alumina powder should be kept between 0.8um and 1um to ensure the reaction and the quality of the final product.
In this embodiment, the heating furnace includes furnace body 1, the material carrying container 2 rotatable mounting is in furnace body 1 bottom, and furnace body 1 is equipped with the actuating mechanism 202 that drives material carrying container 2 rotation outward, material carrying container 2 inner wall is connected with and carries flitch 201, furnace body 1 upper end connect with the nitrogen passage of material carrying container 2 intercommunication, material carrying container 2 inner wall is connected with and carries flitch 201, the gas outlet of nitrogen piping is aimed at material carrying plate 201, when the raw materials ball heats in furnace body 1, actuating mechanism 202 drive material carrying container 2 rotates, seal fit is adopted in the sealed structure that realizes sealing between material carrying container 2 and the furnace body 1 commonly used of industrial rotary kiln: rotary friction sealing, etc., and will not be described in detail here, nitrogen should be continuously introduced into the furnace body 1 during the heating process.
In this embodiment, the nitrogen channel includes an air inlet pipe 101 penetrating through the top of the furnace body 1 and a porous air distribution plate 1011 connected to the lower end of the air inlet pipe 101, an air inlet hole 10111 communicating with the air inlet pipe 101 is provided at the upper end of the porous air distribution plate 1011, a plurality of air outlet holes 10112 are provided at the lower end of the porous air distribution plate 1011, a pyramid 1013 is provided on each air outlet hole 10112, a channel is provided on the pyramid 1013, the channel has an air inlet end 10131 communicating with the air outlet holes 10112 and a plurality of air outlet ends 10132 distributed on the surface of the pyramid 1013, preferably, the material carrying plate 201 is an annular plate, the porous air distribution plate 1011 is a fan-shaped plate, the air inlet hole 10111 of the porous air distribution plate 1011 is provided at the center of the circle, a scraper 1012 is provided at the bottom end of the porous air distribution plate 1011, the scraper 1012 is provided on one straight edge of the porous air distribution plate 1011, and the bottom end height of the scraper 1012 is higher than the height of the pyramid 1013, and the plurality of air outlet ends 10112 are distributed around the arc-shaped path of the porous air distribution plate. The material loading plate 201 is used for containing material balls, after the material balls are put in, the material loading container 2 starts to rotate, the scraping plate 1012 on the porous gas distribution plate 1011 pushes the material balls, so that the material balls form a material layer with uniform thickness on the material loading plate 201, the pyramid 1013 arranged at the rear of the material scraping plate 1012 relative to the advancing direction of the material loading plate 201 breaks the material layer and enters the material layer, meanwhile, nitrogen is introduced into the gas inlet pipeline 101, the nitrogen is ejected from the plurality of gas outlet ends 10132 on the pyramid 1013, under the pushing of the gas flow, the material is reacted, and at the same time, unreacted nitrogen and carbon monoxide gas generated by the reaction push the material balls to continuously roll, so that the nitrogen and various materials are in a flowing and mixing state, all reaction components can fully react, the nitrogen is continuously introduced into the furnace body 1 in the reaction process, a pressure relief valve is arranged on the furnace body 1, and the nitrogen entering the furnace body 1 is discharged by the pressure relief valve.
In this embodiment, the top of the furnace body 1 is perforated with the powder pipe 102, the lower end of the powder pipe 102 is aligned to the top surface of the material carrying plate 201, and when feeding, the raw material balls should not be put into the middle of the material carrying plate 201, so as to ensure that the scraping plate 1012 can scrape all the raw materials into a material layer with uniform thickness in the initial stage.
When the heating furnace of the embodiment is operated, raw materials are put on the material carrying plate 201, the driving mechanism 202 drives the material carrying container 2 to rotate, the scraping plate 1012 on the porous gas distribution plate 1011 pushes the raw material stack to enable the raw material stack to form a raw material layer with uniform thickness, meanwhile, the pyramid 1013 at the lower end of the porous gas distribution plate 1011 enters the raw material layer and injects nitrogen into the raw material layer, the nitrogen pushes the raw materials to roll while reacting with the raw materials, so that the nitrogen and various raw materials are in a flowing and mixing state, each reaction component can fully react, the purity of a product is improved, and the scraping plate 1012 continuously wipes the raw material layer when the material carrying container 2 rotates, so that raw material balls can be continuously turned. Preferably, the rotation speed of the material carrying container 2 is 0.05r/min-0.1r/min so as to ensure the stable progress of the reaction.
While the basic principles and main features of the invention and advantages of the invention have been shown and described, it will be understood by those skilled in the art that the present invention is not limited by the foregoing embodiments, which are described in the foregoing description merely illustrate the principles of the invention, and various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined in the appended claims and their equivalents.
Claims (8)
1. The method for preparing the aluminum nitride powder by the carbothermic method is characterized by comprising the following steps of: comprises the following steps of
S1, preparing raw material balls, mixing alumina and carbon black in proportion, loading the mixture into a ball mill for mixing with grinding materials, sieving, and granulating to obtain the raw material balls for later use;
s2, putting the prepared raw material balls into a heating furnace, wherein a material carrying container is rotatably arranged in the heating furnace, a nitrogen pipeline is communicated with the heating furnace, and the raw material balls are put into the material carrying container;
s3, introducing nitrogen into the heating furnace through a nitrogen pipeline, and starting the heating furnace to heat objects in the furnace, wherein the heating temperature is 1600-1800 ℃ and the heating time is 3 hours;
s4, collecting the reacted product to a carbon removing device, and introducing air into the carbon removing device, wherein the temperature in the carbon removing device is 600-650 ℃;
s5, collecting the product after the reaction in the carbon removal device to obtain the finished aluminum nitride powder.
2. The method for producing aluminum nitride powder by carbothermic process according to claim 1, wherein: the mass ratio of the aluminum oxide to the carbon black is 2:0.6-1.2.
3. The method for producing aluminum nitride powder by carbothermic process according to claim 1, wherein: and adding 11% of aluminum nitride seed crystal and 5% of sintering aid to the raw material ball composed of the aluminum oxide and the carbon black.
4. The method for producing aluminum nitride powder by carbothermic process according to claim 1, wherein: the heating furnace comprises a furnace body, the material carrying container is rotatably arranged at the bottom of the furnace body, a driving mechanism for driving the material carrying container to rotate is arranged outside the furnace body, the inner wall of the material carrying container is connected with a material carrying plate, the upper end of the furnace body is connected with a nitrogen channel communicated with the material carrying container, the inner wall of the material carrying container is connected with a material carrying plate, and the air outlet end of the nitrogen channel is aligned with the material carrying plate.
5. The method for producing aluminum nitride powder by carbothermic process according to claim 4, wherein: the nitrogen channel is including wearing to establish the inlet channel at the furnace body top and connecting the porous gas distribution board at the inlet channel lower extreme, the upper end of porous gas distribution board be equipped with the inlet port of inlet channel intercommunication, the lower extreme of porous gas distribution board is equipped with a plurality of ventholes, every be equipped with the pyramid on the venthole, be equipped with the passageway on the pyramid, the passageway has an inlet end and a plurality of gas outlet ends that distribute on the pyramid surface with the venthole intercommunication.
6. The method for producing aluminum nitride powder by carbothermic process according to claim 5, wherein: the air inlet of the porous air distribution plate is arranged at the center of the circle, the bottom of the porous air distribution plate is provided with a scraping plate, the scraping plate is arranged on one straight edge of the porous air distribution plate, the bottom height of the scraping plate is higher than that of the pyramid, and a plurality of air outlet holes are distributed along a plurality of arc paths around the center of the air distribution plate.
7. The method for producing aluminum nitride powder by carbothermic process according to claim 4, wherein: the top of furnace body wears to be equipped with the powder pipeline, the lower extreme of powder pipeline is aimed at the top surface of year flitch.
8. The method for producing aluminum nitride powder by carbothermic process according to claim 4, wherein: the rotating speed of the material carrying container is 0.05r/min-0.1r/min.
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